Preparative HPLC separations were carried out using a Shimadzu (Kyoto, Japan) system consisting of two LC-8A pumps, a fraction collector (FRC-10A), a SIL-10AP auto sampler, a diode array detector (CPD-M20A) and a CBM-20A communication module. The separations employed a Waters (Milford, MA, USA) PREP Nova-Pak® HR C18 6 μM 60Å 40 × 100 mm reversed phase column with a 40 × 10 mm Guard-Pak insert and a Waters PrepLC Universal Base. The solvent systems employed were MeOH/water gradients both containing 0.1 % TFA or ACN/water gradients also with added 0.1 % TFA. Fractions were collected based on their response at 254 nm.
Sil 10ap autosampler
Manufactured by Shimadzu
Sourced in Japan
The SIL-10AP autosampler is a laboratory instrument designed to automatically introduce samples into an analytical system, such as a gas chromatograph or liquid chromatograph. Its core function is to provide consistent, accurate, and reproducible sample injection, allowing for efficient and high-throughput sample analysis.
Automatically generated - may contain errors
Lab products found in correlation
Lc 8a pump, by Shimadzu (2 mentions)
Frc 10a, by Shimadzu (1 mentions)
Frc 10a fraction collector, by Shimadzu (1 mentions)
Avance dpx 300, by Bruker (1 mentions)
Spd 10av uv vis detector, by Shimadzu (1 mentions)
Avance drx 500, by Bruker (1 mentions)
Lc 20ap pump, by Shimadzu (1 mentions)
Spd m20a, by Shimadzu (1 mentions)
Lc 20ad system, by Shimadzu (1 mentions)
Abz plus column, by Merck Group (1 mentions)
Scl 10a system controller, by Shimadzu (1 mentions)
Rid 10a refractive index detector, by Shimadzu (1 mentions)
5 protocols using sil 10ap autosampler
1
Preparative HPLC Purification of Compounds
2
Synthesis and Purification of Peptide Compounds
3
Preparative Chromatography of Willow Bark Extract
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Preparative chromatography (Figure S5 ) was performed using Shimadzu preparative LC consisting
of two LC-20AP pumps, degasser, SIL-10AP autosampler, SPD-M20A diode
array detector, and FRC-10A fraction collector. The semipreparative
Luna Omega 5 μm PS C18 100 Å (250 × 10 mm) column
and Kinetex 5 μm Biphenyl 100 Å (250 × 10 mm) were
used as a coupled column system for the separation. The bark extract
of willow hybrid Tora was dissolved in water–acetonitrile mixture
(92:8) using a concentration of 5 mg/mL. Ultrapure water–acetonitrile
mixture (9:1) was used as an eluent with a flow rate of 3 mL/min.
A desired fraction of interest (raffinose) was collected from 15 injections
(200 μL/injection) with a retention time of 6.90–7.50
min (Figure S5 ) using a detection wavelength
of 210 nm.
of two LC-20AP pumps, degasser, SIL-10AP autosampler, SPD-M20A diode
array detector, and FRC-10A fraction collector. The semipreparative
Luna Omega 5 μm PS C18 100 Å (250 × 10 mm) column
and Kinetex 5 μm Biphenyl 100 Å (250 × 10 mm) were
used as a coupled column system for the separation. The bark extract
of willow hybrid Tora was dissolved in water–acetonitrile mixture
(92:8) using a concentration of 5 mg/mL. Ultrapure water–acetonitrile
mixture (9:1) was used as an eluent with a flow rate of 3 mL/min.
A desired fraction of interest (raffinose) was collected from 15 injections
(200 μL/injection) with a retention time of 6.90–7.50
min (
of 210 nm.
4
Preparative HPLC Purification of Compounds 1 and 2
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The subfractions F2.3 and F2.5 thus
obtained were repurified by preparative HPLC to obtain compounds1 and 2 , respectively. They were solubilized
in a methanol/ultrapure water mixture (50/50) and then filtered on
polytetrafluoroethylene filters (13 mm; 0.22 μm) (Cloup, Champigny-sur-Marne,
France). Preparative HPLC was performed with an LC-20AD system (Shimadzu,
Kyoto, Japan) equipped with a Shimadzu SIL-10AP autosampler. The separation
column was a SUPELCOSIL ABZ+Plus column (25 cm × 22.1 cm; 5 μm)
(Sigma, St. Louis, Missouri, USA). Elution was performed with a mobile
phase flow rate of 17 mL/min consisting of a mixture of ultrapure
water containing 0.05% formic acid (A) and methanol with 0.05% formic
acid (B); the program started at t = 0 min, ratio
(A/B) 50:50; at t = 20 min, 30:70; at t = 45 min, 5:95; at t = 50 min, 95:5; at t = 55 min, 50:50; and t = 70 min, 50:50.
After purification and drying, 4.3 mg of compound1 and
3.6 mg of compound2 were obtained.
obtained were repurified by preparative HPLC to obtain compounds
in a methanol/ultrapure water mixture (50/50) and then filtered on
polytetrafluoroethylene filters (13 mm; 0.22 μm) (Cloup, Champigny-sur-Marne,
France). Preparative HPLC was performed with an LC-20AD system (Shimadzu,
Kyoto, Japan) equipped with a Shimadzu SIL-10AP autosampler. The separation
column was a SUPELCOSIL ABZ+Plus column (25 cm × 22.1 cm; 5 μm)
(Sigma, St. Louis, Missouri, USA). Elution was performed with a mobile
phase flow rate of 17 mL/min consisting of a mixture of ultrapure
water containing 0.05% formic acid (A) and methanol with 0.05% formic
acid (B); the program started at t = 0 min, ratio
(A/B) 50:50; at t = 20 min, 30:70; at t = 45 min, 5:95; at t = 50 min, 95:5; at t = 55 min, 50:50; and t = 70 min, 50:50.
After purification and drying, 4.3 mg of compound
3.6 mg of compound
5
Preparative HPLC for Carbohydrate Purification
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The preparative HPLC system consisted of two high-pressure gradient Shimadzu LC-8A pumps with a 150 mL/min pump head, a Shimadzu preparative 14 mL mixing chamber, Shimadzu SIL 10AP autosampler, Shimadzu RID 10A refractive index detector, and a Shimadzu SCL 10A system controller. Shimadzu Class VP software v. 6.12SP5 was used for operating the system and for data acquisition.
A 50 × 800 mm column packed with BioGel P2 Gel fine grade (Bio-Rad, Valimotie, Finland) was used at 5.0 mL/min isocratic 0.1 M acetic acid flow. Fractions were collected automatically based on pre-determined retention time. After chromatographic separation, the collected fractions were evaporated to dryness yielding an amorphous solid.
Subsequently, esterification was carried out prior to NMR analysis in analogy to the raffinose model compound. The product obtained appeared as a colorless, viscous liquid and was directly dissolved in NMR solvent for analysis.
A 50 × 800 mm column packed with BioGel P2 Gel fine grade (Bio-Rad, Valimotie, Finland) was used at 5.0 mL/min isocratic 0.1 M acetic acid flow. Fractions were collected automatically based on pre-determined retention time. After chromatographic separation, the collected fractions were evaporated to dryness yielding an amorphous solid.
Subsequently, esterification was carried out prior to NMR analysis in analogy to the raffinose model compound. The product obtained appeared as a colorless, viscous liquid and was directly dissolved in NMR solvent for analysis.
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